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Quantification of neomangiferin in rat plasma by liquid chromatography-tandem mass spectrometry and its application to bioavailability study$

Bo YANG ; Zhirui LIU ; Shenglan SHANG ; Xiaojian QIN ; Peiyuan XIA

Journal of Pharmaceutical Analysis.2015;5(5):335-340.

Neomangiferin, a natural C-glucosyl xanthone, has recently received a great deal of attention due to its multiple biological activities. In this study, a rapid and sensitive ultra-high performance liquid chroma-tography tandem mass spectrometry (UHPLC–MS/MS) method for the quantification of neomangiferin in rat plasma was developed. Using chloramphenicol as an internal standard (IS), plasma samples were subjected to a direct protein precipitation process using methanol (containing 0.05% formic acid). Quan-tification was performed by multiple reactions monitoring (MRM) method, with the transitions of the parent ions to the product ions of m/z 583.1-330.9 for NG and m/z 321.1-151.9 for IS. The assay was shown to be linear over the range of 0.2–400 ng/mL, with a lower limit of quantification of 0.2 ng/mL. Mean recovery of neomangiferin in plasma was in the range of 97.76%–101.94%. Relative standard deviations (RSDs) of intra-day and inter-day precision were both o 10%. The accuracy of the method ranged from 94.20%to 108.72%. This method was successfully applied to pharmacokinetic study of neomangiferin after intravenous (2 mg/kg) and intragastric (10 mg/kg) administration for the first time. The oral absolute bioavailability of neomangiferin was estimated to be 0.53%7 0.08%with an elimination half-life (t1/2) value of 2.74 7 0.92 h, indicating its poor absorption and/or strong metabolism in vivo.

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Pharmacokinetics of gene recombined angiogenesis inhibitor Kringle 5 in vivo using 131I specific markers and SPECT/CT$

Ge YAN ; Danrong YANG ; Yan YU ; Jianjun XUE ; Yifan JIA ; Xuanzi SUN ; Boyu WANG ; Zewei ZHAO ; Maode WANG

Journal of Pharmaceutical Analysis.2015;5(5):313-317.

The previous pharmacokinetic methods can be only limited to drug analysis in vitro, which provide less information on the distribution and metabolismof drugs, and limit the interpretation and assessment of pharmacokinetics, the determination of metabolic principles, and evaluation of treatment effect. The objective of the study was to investigate the pharmacokinetic characteristics of gene recombination angiogenesis inhibitor Kringle 5 in vivo. The SPECT/CT and specific 131I-Kringle 5 marked by Iodogen method were both applied to explore the pharmacokinetic characteristics of 131I-Kringle 5 in vivo, and to investigate the dynamic distributions of 131I-Kringle 5 in target organs. Labeling recombinant angio-genesis inhibitor Kringle 5 using 131I with longer half-life and imaging in vivo using SPECT instead of PET, could overcome the limitations of previous methods. When the doses of 131I-Kringle 5 were 10.0, 7.5 and 5.0 g/kg, respectively, the two-compartment open models can be determined within all the metabolic process in vivo. There were no significant differences in t1/2α, t1/2β, apparent volume of distribution and CL between those three levels. The ratio of AUC(0 ? 1) among three different groups of 10.0, 7.5 and 5.0 g/kg was 2.56:1.44:1.0, which was close to the ratio (2:1.5:1.0). It could be clear that in the range of 5.0–10.0 g/kg, Kringle 5 was characterized by the first-order pharmacokinetics. Approximately 30 min after 131I-Kringle 5 was injected, 131I-Kringle 5 could be observed to concentrate in the heart, kidneys, liver and other organs by means of planar imaging and tomography. After 1 h of being injected, more radionuclide retained in the bladder, but not in intestinal. It could be concluded that 131I-Kringle 5 is mainly excreted through the kidneys. About 2 h after the injection of 131I-Kringle 5, the radionuclide in the heart, kidneys, liver and other organs was gradually reduced, while more radionuclide was concentrated in the bladder. The radionuclide was completely metabolized within 24 h, and the distribution of radioactivity in rats was similar to normal levels. In our study, the specific marker 131I-Kringle 5 and SPECT/CT were suc-cessfully used to explore pharmacokinetic characteristics of Kringle 5 in rats. The study could provide a new evaluation platform of the specific, in vivo and real-time functional imaging and pharmacokinetics for the clinical application of 131I-Kringle 5.

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Inclusion complexes of cefuroxime axetil withβ-cyclodextrin:Physicochemical characterization, molecular modeling and effect of L-arginine on complexation$

Sarika SAPTE ; Yogesh PORE

Journal of Pharmaceutical Analysis.2015;5(5):300-306.

The inclusion complexes of poorly water-soluble cephalosporin, cefuroxime axetil (CFA), were prepared withβ-cyclodextrin (βCD) with or without addition of L-arginine (ARG) to improve its physicochemical properties. We also investigated the effect of ARG on complexation efficiency (CE) ofβCD towards CFA in an aqueous medium through phase solubility behaviour according to Higuchi and Connors. Although phase solubility studies showed AL (linear) type of solubility curve in presence and absence of ARG, the CE and association constant (Ks) ofβCD towards CFA were significantly promoted in presence of ARG, justifying its use as a ternary component. The solid systems of CFA withβCD were obtained by spray drying technique with or without incorporation of ARG and characterized by differential scanning ca-lorimetry (DSC), X-ray powder diffractometry (XRPD), scanning electron microscopy (SEM), and sa-turation solubility and dissolution studies. The molecular modeling studies provided a better insight into geometry and inclusion mode of CFA insideβCD cavity. The solubility and dissolution rate of CFA were significantly improved upon complexation withβCD as compared to CFA alone. However, ternary system incorporated with ARG performed better than binary system in physicochemical evaluation. In conclu-sion, ARG could be exploited as a ternary component to improve the physicochemical properties of CFA viaβCD complexation.

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Detection of phthalates migration from disposable tablewares to drinking water using hexafluoroisopropanol-induced catanionic surfactant coacervate extraction$

Cao LI ; Jia XU ; Dan CHEN ; Yuxiu XIAO

Journal of Pharmaceutical Analysis.2015;5(5):292-299.

Hexafluoroisopropanol (HFIP)-induced sodium dodecyl sulfate/dodecyltrimethylammonium bromide (SDS/DTAB) catanionic surfactant coacervate extraction method coupled with high performance liquid chromatography (HPLC) was used to detect the migration of phthalates from disposable tablewares to drinking water. The concentration factors are larger than 82 and extraction recoveries over 53%for water samples spiked with 100 or 200 ng/mL phthalates. Limit of detection is in the range of 1.0–2.6 ng/mL. Good linearity with correlation coefficients larger than 0.9985 is obtained in the concentration of 20–1500 or 40–3000 ng/mL. Relative recoveries are from 82.4%to 123.6%for water samples spiked with 30/60, 250/500, and 1500/3000 ng/mL phthalates, respectively. Relative standard deviations (RSDs) are 0.4%–7.4% for intraday precision (n ? 5) and 0.6%–7.8% for interday precision (n ? 3). Four of studied phthalates are found in the drinking water samples prepared from four kinds of tablewares.

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Optimization of high pressure machine decocting process for Dachengqi Tang using HPLC fingerprints combined with the Box-Behnken experimental design

Ruifang XIE ; Zhina SHI ; Zhicheng LI ; Peipei CHEN ; Yimin LI ; Xin ZHOU

Journal of Pharmaceutical Analysis.2015;(2):110-119. doi:10.1016/j.jpha.2014.07.001

Using Dachengqi Tang (DCQT) as a model, high performance liquid chromatography (HPLC) fingerprints were applied to optimize machine extracting process with the Box–Behnken experimental design. HPLC fingerprints were carried out to investigate the chemical ingredients of DCQT; synthetic weighing method based on analytic hierarchy process (AHP) and criteria importance through intercriteria correlation (CRITIC) was performed to calculate synthetic scores of fingerprints; using the mark ingredients contents and synthetic scores as indicators, the Box–Behnken design was carried out to optimize the process parameters of machine decocting process under high pressure for DCQT. Results of optimal process showed that the herb materials were soaked for 45 min and extracted with 9 folds volume of water in the decocting machine under the temperature of 140 1C till the pressure arrived at 0.25 MPa;then hot decoction was excreted to soak Dahuang and Mangxiao for 5 min. Finally, obtained solutions were mixed, filtrated and packed. It concluded that HPLC fingerprints combined with the Box–Behnken experimental design could be used to optimize extracting process of traditional Chinese medicine (TCM).

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Simultaneous determination of four active components in Alisma orientale (Sam.) Juz. by HPLC-DAD using a single reference standard

Yaowen ZHANG ; Qing LI ; Chunxiao LV ; Xiujia LIU ; Xiaohui CHEN ; Kaishun BI

Journal of Pharmaceutical Analysis.2015;(2):85-92. doi:10.1016/j.jpha.2014.12.001

A rapid, simple and practical high-performance liquid chromatography method coupled with diode array detector (HPLC–DAD) was developed to evaluate the quality of Alisma orientale (Sam.) Juz. through a simultaneous determination of four major active triterpenes using a single standard to determine the multi-components (SSDMCs). Alisol B 23-acetate was selected as the reference compound for calculating the relative response factors. All calibration curves showed good linearity (R240.9998) within test ranges. RSDs for intra- and inter-day of four analytes were less than 3.6% and 2.3%; the overall recovery was 92.1–110.2%(SSDMC). The proposed method was successfully applied to quantify the four components in 20 samples from different localities in China. Moreover, significant variations were demonstrated in the content of these compounds. In addition, hierarchical clustering analysis (HCA) and principal components analysis (PCA) were performed to differentiate and classify the samples based on the contents of Alisol C 23-acetate, Alisol A, Alisol A 24-acetate and Alisol B 23-acetate. This simple, rapid, low-cost and reliable HPLC–DAD method using SSDMC is suitable for routine quantitative analysis and quality control of A. orientale (Sam.) Juz.

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Liquid chromatography-tandem mass spectrometry method for the estimation of adefovir in human plasma：Application to a pharmacokinetic study

Dipanjan GOSWAMI ; Sanjay GURULE ; Arabinda SAHA ; Poonam VATS ; Arshad KHUROO ; Tausif MONIF

Journal of Pharmaceutical Analysis.2015;(3):190-199.

An analytical method based on solid phase extraction was developed and validated for analysis of adefovir in human plasma. Adefovir-d4 was used as an internal standard and Synergi MAX RP80A (150 mm × 4.6 mm, 4μm) column provided the desired chromatographic separation of compounds followed by detection with mass spectrometry. The method used simple isocratic chromato-graphic condition and mass spectrometric detection in the positive ionization mode. The calibration curves were linear over the range of 0.50–42.47 ng/mL with the lower limit of quantitation validated at 0.50 ng/mL. Matrix effect was assessed by post-column infusion experiment to monitor phospholipids and post-extraction addition experiment was performed. The degree of matrix effect for adefovir was determined as 7.5%and ion-enhancement in five different lots of human plasma was 7.1%and had no impact on study samples analysis with 4.5 min run time. The intra- and inter-day precision values were within 7.7% and 7.8%, respectively, for adefovir at the lower limit of quantification level. Validated bioanalytical method was successfully applied to clinical sample analysis.

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Determination of diclofenac in pharmaceutical preparations by voltammetry and gas chromatography methods

Bilal YILMAZ ; Ulvihan CILTAS

Journal of Pharmaceutical Analysis.2015;(3):153-160.

Rapid, sensitive and specific methods were developed for the determination of diclofenac in pharmaceutical preparations by linear sweep voltammetry (LSV) and gas chromatography (GC) with mass spectrometry (MS) detection. The linearity was established over the concentration range of 5–35μg/mL for LSV and 0.25–5μg/mL for GC–MS method. The intra- and inter-day relative standard deviation (RSD) was less than 4.39% and 4.62% for LSV and GC–MS, respectively. Limits of quantification (LOQ) were determined as 4.8 and 0.15μg/mL for LSV and GC–MS, respectively. No interference was found from tablet excipients at the selected assay conditions. The methods were applied for the quality control of commercial diclofenac dosage forms to quantify the drug and to check the formulation content uniformity.

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Isolation and characterization of a degradation product in leflunomide and a validated selective stability-indicating HPLC-UV method for their quantification

Balraj SAINI ; Gulshan BANSAL

Journal of Pharmaceutical Analysis.2015;(3):207-212.

Leflunomide (LLM) is subjected to forced degradation under conditions of hydrolysis, oxidation, dry heat, and photolysis as recommended by International Conference on Harmonization guideline Q1A(R2). In total, four degradation products (I–IV) were formed under different conditions. Products I, II and IV were formed in alkaline hydrolytic, acidic hydrolytic and alkaline photolytic conditions. LLM and all degradation products were optimally resolved by gradient elution over a C18 column. The major degradation product (IV) formed in hydrolytic alkaline conditions was isolated through column chromatography. Based on its 1H NMR, IR and mass spectral data, it was characterized as a British Pharmacopoeial impurity B. The HPLC method was found to be linear, accurate, precise, sensitive, specific, rugged and robust for quantification of LLM as well as product IV. Finally, the method was applied to stability testing of the commercially available LLM tablets.

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Selective extraction of dimethoate from cucumber samples by use of molecularly imprinted microspheres

Jiaojiao DU ; Ruixia GAO ; Hu YU ; Xiaojing LI ; Hui MU

Journal of Pharmaceutical Analysis.2015;(3):200-206.

Molecularly imprinted polymers for dimethoate recognition were synthesized by the precipitation polymerization technique using methyl methacrylate (MMA) as the functional monomer and ethylene glycol dimethacrylate (EGDMA) as the cross-linker. The morphology, adsorption and recognition properties were investigated by scanning electron microscopy (SEM), static adsorption test, and competitive adsorption test. To obtain the best selectivity and binding performance, the synthesis and adsorption conditions of MIPs were optimized through single factor experiments. Under the optimized conditions, the resultant polymers exhibited uniform size, satisfactory binding capacity and significant selectivity. Furthermore, the imprinted polymers were successfully applied as a specific solid-phase extractants combined with high performance liquid chromatography (HPLC) for determination of dimethoate residues in the cucumber samples. The average recoveries of three spiked samples ranged from 78.5% to 87.9% with the relative standard deviations (RSDs) less than 4.4% and the limit of detection (LOD) obtained for dimethoate as low as 2.3μg/mL.

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